分散固相萃取-气相色谱-串联质谱法测定铁皮石斛中41种农药的残留量
|
摘要
适量水浸润的铁皮石斛样品经乙腈高速涡旋和超声提取。离心后,上清液采用分散固相萃取净化,吸附剂为C18和N-丙基乙二胺。采用分散固相萃取-气相色谱-串联质谱法测定净化液中41种农药的残留量。在气相色谱分离中采用Agilent VF-5MS色谱柱,在串联质谱分析中采用多反应监测模式。以外环氧七氯为内标,41种农药的检出限(3S/N)为0.001～0.024 mg·kg~(-1)。以空白样品为基体进行加标回收试验,所得回收率为75.1%～115%,测定值的相对标准偏差(n=6)为0.40%～11%。
The dendrobium candidum sample soaked with appropriate amount water was extracted ultrasonically with acetonitrile accompanied by high speed vortex.After centrifugation,the supernatant was purified with dispersive solid phase extraction.C18 and PSA were used as adsorbents.GC-MS/MS was applied to the determination of residual amounts of 41 pesticides in purified liquid with dispersive solid phase extraction.Agilent VF-5 MS chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS/MS determination.cis-Heptachlor epoxide was used as internal standard.Detection limits(3 S/N)of the 41 pesticides were in the range of 0.001-0.024 mg·kg~(-1).On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 75.1%~(-1)15%,with RSDs(n=6)of determined values in the range of 0.40%~(-1)1%.
The dendrobium candidum sample soaked with appropriate amount water was extracted ultrasonically with acetonitrile accompanied by high speed vortex.After centrifugation,the supernatant was purified with dispersive solid phase extraction.C18 and PSA were used as adsorbents.GC-MS/MS was applied to the determination of residual amounts of 41 pesticides in purified liquid with dispersive solid phase extraction.Agilent VF-5 MS chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS/MS determination.cis-Heptachlor epoxide was used as internal standard.Detection limits(3 S/N)of the 41 pesticides were in the range of 0.001-0.024 mg·kg~(-1).On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 75.1%~(-1)15%,with RSDs(n=6)of determined values in the range of 0.40%~(-1)1%.
引文
[1]陈晓梅,郭顺星.石斛属植物化学成分和药理作用的研究进展[J].天然产物研究与开发,2001,13(1):70-75.
[2]林萍,毕志明,徐红,等.石斛属植物药理活性研究进展[J].中草药,2003,34(11):1073-1076.
[3]国家药典委员会.中华人民共和国药典(四部)[M].北京:中国医药科技出版社,2015.
[4]蒋雪松,王维琴,许林云,等.农产品/食品中农药残留快速检测方法研究进展[J].农业工程学报,2016,32(20):267-274.
[5]王吉祥,王亚琴,牛之瑞,等.GC-MS/MS法测定铁皮石斛中19种农药残留[J].食品研究与开发,2016,37(7):131-135.
[6]吴永江,朱炜,程翼宇,等.液-质联用法测定铁皮石斛和西洋参及制剂中多菌灵残留[J].分析化学,2006,34(2):235-238.
[7]方翠芬,谭春梅,马临科,等.HPLC/MS/MS测定铁皮石斛制剂中12种农药残留量[J].医药导报,2012,31(11):1481-1484.
[8]胡奇杰,朱佳茜,王新财,等.铁皮石斛饮片中有机氯及拟除虫菊酯农药多残留检测方法的研究[J].安徽农业科学,2016,44(7):66-69.
[9]虞淼,梁赤周,唐芬芬,等.HPLC/MS/MS测定铁皮石斛中咪鲜胺的残留[J].农药科学与管理,2016,37(7):34-37.
[10]张仙,王小飞,彭西甜,等.改良QuEChERS-气相色谱法测定韭菜中15种有机磷农药残留[J].湖北农业科学,2017,56(10):1941-1944.
[11]孙志高,盛冉,郝静梅,等.QuEChERS-高效液相色谱法检测柑桔中毒死蜱、吡虫啉和残杀威农残[J].食品与机械,2017,33(6):68-72.
[12]崔如玉,李壹,熊晓辉.食品中常见有机磷农药残留的气相色谱质谱检测方法[J].南京工业大学学报(自然科学版),2017,39(1):137-144.
[13]施家威,李继革,王玉飞,等.固相萃取-气相色谱/三重四极杆串联质谱分析蔬菜中42种农药残留[J].色谱,2010,28(12):1137-1143.
[14]沈伟健,余可垚,桂茜雯,等.分散固相萃取-气相色谱-串联质谱法测定蔬菜中107种农药的残留量[J].色谱,2009,27(4):391-400.
[15]孙磊丽,李晓玉,隋涛.气相色谱-串联质谱测定菠菜中有机氯残留量[J].广州化工,2010,38(11):155-157.
[16]易盛国,侯雪,韩梅,等.气相色谱-串联质谱法检测蔬菜农药残留基质效应与基质分类的研究[J].西南农业学报,2012,25(2):537-543.
[17]宋淑玲,李重九,马晓东,等.蔬菜中残留农药的石墨化碳黑净化和气相色谱-质谱检测方法[J].分析化学,2008,36(11):1526-1530.
[18]叶华夏,谢正敏,张倩,等.气相色谱-三重四级杆质谱联用法测定酿酒用原辅料中108种农药残留[J].酿酒科技,2017,271(1):102-107.
[19]吴俐,曹赵云,陈铭学,等.气相色谱-串联质谱测定水稻中10种拟除虫菊酯类杀虫剂农药残留[J].安徽农业科学,2017,45(6):147-150.
[20]孙华庚,王媚,赵爱源,等.气相色谱-质谱法测定东北人参中9种农药残留[J].食品研究与开发,2017,38(6):116-120.
[21]罗彦波,郑浩博,姜兴益,等.在线凝胶渗透色谱-气相色谱-串联质谱联用检测烟叶中的农药残留[J].分析化学,2015,43(10):1538-1544.
[22]王立闱,范军,吴国华,等.在线凝胶色谱-串联三重四极杆质谱法测定大豆油中42种农药残留[J].质谱学报,2016,37(4):374-384.
[23]王连珠,周昱,陈泳,等.QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估[J].色谱,2012,30(2):146-153.
[2]林萍,毕志明,徐红,等.石斛属植物药理活性研究进展[J].中草药,2003,34(11):1073-1076.
[3]国家药典委员会.中华人民共和国药典(四部)[M].北京:中国医药科技出版社,2015.
[4]蒋雪松,王维琴,许林云,等.农产品/食品中农药残留快速检测方法研究进展[J].农业工程学报,2016,32(20):267-274.
[5]王吉祥,王亚琴,牛之瑞,等.GC-MS/MS法测定铁皮石斛中19种农药残留[J].食品研究与开发,2016,37(7):131-135.
[6]吴永江,朱炜,程翼宇,等.液-质联用法测定铁皮石斛和西洋参及制剂中多菌灵残留[J].分析化学,2006,34(2):235-238.
[7]方翠芬,谭春梅,马临科,等.HPLC/MS/MS测定铁皮石斛制剂中12种农药残留量[J].医药导报,2012,31(11):1481-1484.
[8]胡奇杰,朱佳茜,王新财,等.铁皮石斛饮片中有机氯及拟除虫菊酯农药多残留检测方法的研究[J].安徽农业科学,2016,44(7):66-69.
[9]虞淼,梁赤周,唐芬芬,等.HPLC/MS/MS测定铁皮石斛中咪鲜胺的残留[J].农药科学与管理,2016,37(7):34-37.
[10]张仙,王小飞,彭西甜,等.改良QuEChERS-气相色谱法测定韭菜中15种有机磷农药残留[J].湖北农业科学,2017,56(10):1941-1944.
[11]孙志高,盛冉,郝静梅,等.QuEChERS-高效液相色谱法检测柑桔中毒死蜱、吡虫啉和残杀威农残[J].食品与机械,2017,33(6):68-72.
[12]崔如玉,李壹,熊晓辉.食品中常见有机磷农药残留的气相色谱质谱检测方法[J].南京工业大学学报(自然科学版),2017,39(1):137-144.
[13]施家威,李继革,王玉飞,等.固相萃取-气相色谱/三重四极杆串联质谱分析蔬菜中42种农药残留[J].色谱,2010,28(12):1137-1143.
[14]沈伟健,余可垚,桂茜雯,等.分散固相萃取-气相色谱-串联质谱法测定蔬菜中107种农药的残留量[J].色谱,2009,27(4):391-400.
[15]孙磊丽,李晓玉,隋涛.气相色谱-串联质谱测定菠菜中有机氯残留量[J].广州化工,2010,38(11):155-157.
[16]易盛国,侯雪,韩梅,等.气相色谱-串联质谱法检测蔬菜农药残留基质效应与基质分类的研究[J].西南农业学报,2012,25(2):537-543.
[17]宋淑玲,李重九,马晓东,等.蔬菜中残留农药的石墨化碳黑净化和气相色谱-质谱检测方法[J].分析化学,2008,36(11):1526-1530.
[18]叶华夏,谢正敏,张倩,等.气相色谱-三重四级杆质谱联用法测定酿酒用原辅料中108种农药残留[J].酿酒科技,2017,271(1):102-107.
[19]吴俐,曹赵云,陈铭学,等.气相色谱-串联质谱测定水稻中10种拟除虫菊酯类杀虫剂农药残留[J].安徽农业科学,2017,45(6):147-150.
[20]孙华庚,王媚,赵爱源,等.气相色谱-质谱法测定东北人参中9种农药残留[J].食品研究与开发,2017,38(6):116-120.
[21]罗彦波,郑浩博,姜兴益,等.在线凝胶渗透色谱-气相色谱-串联质谱联用检测烟叶中的农药残留[J].分析化学,2015,43(10):1538-1544.
[22]王立闱,范军,吴国华,等.在线凝胶色谱-串联三重四极杆质谱法测定大豆油中42种农药残留[J].质谱学报,2016,37(4):374-384.
[23]王连珠,周昱,陈泳,等.QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估[J].色谱,2012,30(2):146-153.